盐酸氨基葡萄糖片中5-HMF的含量测定及形成动力学研究  

Content determination of 5-HMF in glucosamine hydrochloride tablets and formation kinetics study

作　　者：倪东宇 王琼芬 张梦奇 李彬 石婧 徐虹 张帅 NI Dongyu;WANG Qiongfen;ZHANG Mengqi;LI Bin;SHI Jing;XU Hong;ZHANG Shuai(College of Food and Pharmacy,Zhejiang Ocean University,Zhejiang Zhoushan 316022,China;Zhoushan Institute for Food and Drug Control,Zhejiang Zhoushan 316021,China)

机构地区：[1]浙江海洋大学食品与药学学院,浙江舟山316022 [2]舟山市食品药品检验检测研究院,浙江舟山316021

出　　处：《中国药房》2023年第8期950-954,共5页China Pharmacy

基　　金：浙江省药品监管系统科技计划项目(No.2021004)。

摘　　要：目的 建立测定盐酸氨基葡萄糖片中5-羟甲基糠醛(5-HMF)含量的方法,分析其含量变化规律及影响因素。方法 采用高效液相色谱法对5-HMF进行定量测定,以Shim-pack GIST C18-AQ为色谱柱,0.1%磷酸溶液-甲醇(90∶10,V/V)为流动相,柱温为30℃,检测波长为284 nm,流速为1.0 mL/min,进样量为20μL。通过不同温度反应动力学实验分析5-HMF含量与反应温度、反应时间的相关性,建立其形成动力学模型。结果 5-HMF检测质量浓度的线性范围为0.057~5.698μg/mL(r=0.999 9);检测限为5.70 ng/mL,定量限为17.09 ng/mL;精密度、重复性和稳定性(24 h)试验的RSD均小于1.0%(n=6);加样回收率为99.38%~99.73%(RSD=0.53%,n=9)。8批样品含量为4.10~35.13μg/g。反应动力学实验数据拟合结果显示,随着反应温度升高、反应时间延长,样品中5-HMF含量越高。50、60、70、80℃下,5-HMF含量与反应时间均呈线性关系,符合零级动力学模型,反应速率常数分别为6.789、7.715、8.815、11.430。结论 所建含量测定方法专属性强、灵敏度高、准确度好;反应温度和反应时间是影响盐酸氨基葡萄糖片中5-HMF形成的重要因素,其含量变化规律符合零级动力学模型。OBJECTIVE To establish the method for the content determination of 5-hydroxymethylfurfural(5-HMF)in glucosamine hydrochloride tablets,and to analyze its regularity and influential factors.METHODS Quantitative analysis of 5-HMF was performed using high-performance liquid chromatography.The analysis was conducted on Shim-pack GIST C18-AQ column with mobile phase consisted of 0.1%phosphoric acid solution-methanol(90∶10,V/V)at the flow rate of 1.0 mL/min.The column temperature was 30℃,and detection wavelength was 284 nm.The injection volume was 20μL.Reaction kinetics test of different temperatures was adopted to analyze the relationship of 5-HMF content with reaction temperature and reaction time,and utilized to build its formation kinetic model.RESULTS The linger range of 5-HMF was 0.057-5.698μg/mL(r=0.9999).The limits of detection and quantitation were 5.70 and 17.09 ng/mL;RSDs of precision,repeatability and stability(24 h)tests were all lower than 1.0%(n=6).The average recoveries ranged from 99.38%to 99.73%(RSD=0.53%,n=9).The contents of the 5-HMF in 8 batches of samples ranged 4.10-35.13μg/g.Results of data fitting in reaction kinetics test showed that the higher reaction temperature and the longer reaction time,the higher 5-HMF content in the sample.At 50,60,70 and 80℃,the relationship between the content of 5-HMF and the reaction time was linear,in accordance with a zero-order kinetic model.The reaction rate constants were 6.789,7.715,8.815 and 11.430,respectively.CONCLUSIONS The established method has strong specificity,high sensitivity,and good accuracy;the reaction temperature and reaction time are important influential factors for the formation of 5-HMF in glucosamine hydrochloride tables.The change rule of its content conforms to the zero-order kinetic model.

关 键 词：盐酸氨基葡萄糖片 5-羟甲基糠醛 高效液相色谱法 含量测定 形成动力学 

分 类 号：R917[医药卫生—药物分析学]